CN108117665A - Plate resistor unleaded encasement medium slurry of anti-acid and preparation method thereof - Google Patents
Plate resistor unleaded encasement medium slurry of anti-acid and preparation method thereof Download PDFInfo
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- CN108117665A CN108117665A CN201711370188.9A CN201711370188A CN108117665A CN 108117665 A CN108117665 A CN 108117665A CN 201711370188 A CN201711370188 A CN 201711370188A CN 108117665 A CN108117665 A CN 108117665A
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- Prior art keywords
- acid
- unleaded
- plate resistor
- medium slurry
- glass dust
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
- H01C17/02—Apparatus or processes specially adapted for manufacturing resistors adapted for manufacturing resistors with envelope or housing
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses it is a kind of by comprising the plate resistor that lead-free glass powder, inorganic additive and organic carrier are formed with unleaded encasement medium slurry of anti-acid, wherein the glass dust is Bi Ca Si Zn systems, percentage composition Bi by weight2O330% ~ 50%, CaO 15% ~ 20%, SiO218% ~ 25%, ZnO 10% ~ 20%, B2O33% ~ 10%, wherein the inorganic additive is Al2O3、ZnO、ZrO2And TiO2In one or several kinds.It it is an advantage of the invention that having invented a kind of lead-free glass powder, solves the acidproof sex chromosome mosaicism of a medium packaging slurry, while has the characteristics that encapsulating change rate is small.
Description
Technical field
The invention belongs to dielectric paste technical fields, and in particular to a kind of plate resistor once encapsulates Jie with unleaded anti-acid
Chylema material and preparation method thereof.
Background technology
Chip resistor main application fields are mobile phone, household electrical appliances, camera, communication equipment, automotive electronics, LED etc., at present
The sales volume in the whole world is also increased at monthly 150,000,000,000 with 10% speed every year.
Packaging slurry product of plate resistor of domestic several large manufacturers relies primarily on external product at present, and the country does not have
Corresponding electric slurry manufacturer, this seriously constrains the development of plate resistor industry, therefore for plate resistor with once wrapping
The research and development of slurry seal material just seem especially urgent and necessary.
During plate resistor is electroplated, plate resistor is with an encasement medium slurry by acidic Bath
When, what acid solution can be directly or indirectly is contacted with a packaging slurry, so as to destroy plate resistor product, it is therefore necessary to possess
Good acid resistance.
Therefore, research and development are a kind of has acid resistance simultaneously, and is capable of providing excellent printing, the encapsulating variation of very little
Rate, adapting to an encasement medium slurry of plate resistor miniaturization trend is necessary.
The content of the invention
In view of this, it is a primary object of the present invention to provide plate resistor with unleaded encasement medium slurry of anti-acid
And preparation method thereof.
In order to achieve the above objectives, the technical proposal of the invention is realized in this way:
The unleaded encasement medium slurry of anti-acid of plate resistor, it is characterized in that:Percentage composition by weight, including following
Component,
Glass dust 60%~75%, inorganic additive 2%~5%, organic carrier 20%~35%.
The glass dust is Bi-Ca-Si-Zn systems.
Percentage composition by weight, the glass dust include Bi2O330%~50%, CaO 15%~20%, SiO218%~
25%th, ZnO 10%~20% and B2O33%~10%.
The inorganic additive is Al2O3、ZnO、ZrO2Or TiO2In one or several kinds.
Percentage composition by weight, the organic carrier include resin 4%~16%, organic additive 1%~4% and organic
Solvent 60%~90%.
The resin is one or more of rosin resin, ethyl cellulose or methylcellulose.
The organic solvent is one or both of alcohols or ethers mixture.
The preparation method of the unleaded encasement medium slurry of anti-acid of plate resistor, which is characterized in that specifically include with
Lower step:
1) glass dust is prepared
Percentage composition by weight, by Bi2O330%~50%, CaO 15%~20%, SiO218%~25%, ZnO
10%~20% and B2O33%~10% weigh after be sufficiently mixed with three-dimensional material mixer, with corundum crucible Sheng take after 1000 DEG C~
It is melted under the conditions of 1500 DEG C, molten liquid is poured into, water quenching is carried out in deionized water at normal temperature, finally by the glass dregs after water quenching
Glass dust finished product is obtained after ball milling, drying, a series of processing of sieving;
2) inorganic additive is prepared
The inorganic additive is Al2O3、ZnO、ZrO2Or TiO2In one or several kinds, granularity be less than 8 μm, preferably
Particle size range is 0.5~5 μm;
3) organic carrier is prepared
Percentage composition, the organic carrier it will include resin 4%~16%, organic additive 1%~4% by weight and have
Solvent 60%~90% is dissolved and modulated at 50-150 DEG C, and preferable temperature is 60 DEG C~90 DEG C;
4) plate resistor is prepared with unleaded encasement medium slurry of anti-acid
Above-mentioned glass dust, inorganic additive are dispersed in by stirring, rolling in organic carrier, have half so as to be prepared into
The unleaded encasement medium slurry of anti-acid of plate resistor is made in the dispersion of fluid viscosity.
Compared with prior art, beneficial effects of the present invention:
Plate resistor provided by the invention has acid resistance with unleaded encasement medium slurry of anti-acid, and can carry
For excellent printing, there is the encapsulating change rate of very little, and adapt to plate resistor miniaturization trend.Its raw material is simple
Be easy to get, technological process facilitate it is easy to control, suitable for the product demand of multiple performance.
Specific embodiment
The present invention will be described in detail With reference to embodiment.
The present invention provides a kind of unleaded encasement medium slurry of anti-acid of plate resistor, specifically, percentage by weight
Content, including following components,
Glass dust 60%~75%, inorganic additive 2%~5%, organic carrier 20%~35%.
The glass dust is Bi-Ca-Si-Zn systems.
Percentage composition by weight, the glass dust include Bi2O330%~50%, CaO 15%~20%, SiO218%~
25%th, ZnO 10%~20% and B2O33%~10%.
The inorganic additive is Al2O3、ZnO、ZrO2Or TiO2In one or several kinds.
Percentage composition by weight, the organic carrier include resin 4%~16%, organic additive 1%~4% and organic
Solvent 60%~90%.
The resin is one or more of rosin resin, ethyl cellulose or methylcellulose.
The organic solvent is one or both of alcohols or ethers mixture.
The preparation method of the unleaded encasement medium slurry of anti-acid of plate resistor, which is characterized in that specifically include with
Lower step:
1) glass dust is prepared
Percentage composition by weight, by Bi2O330%~50%, CaO 15%~20%, SiO218%~25%, ZnO
10%~20% and B2O33%~10% weigh after be sufficiently mixed with three-dimensional material mixer, with corundum crucible Sheng take after 1000 DEG C~
It is melted under the conditions of 1500 DEG C, molten liquid is poured into, water quenching is carried out in deionized water at normal temperature, finally by the glass dregs after water quenching
Glass dust finished product is obtained after ball milling, drying, a series of processing of sieving;
2) inorganic additive is prepared
The inorganic additive is Al2O3、ZnO、ZrO2Or TiO2In one or several kinds, granularity be less than 8 μm, preferably
Particle size range is 0.5~5 μm;Selected inorganic additive is CP grades of reagents, inorganic to meet the net of crossing when slurry prints
The granularity of additive is less than 8 μm, so needing that inorganic additive is carried out to add mill and grading processing, preferred size scope is
0.5~5 μm;
3) organic carrier is prepared
Percentage composition, the organic carrier it will include resin 4%~16%, organic additive 1%~4% by weight and have
Solvent 60%~90% is dissolved and modulated at 50-150 DEG C, and preferable temperature is 60 DEG C~90 DEG C;Due to low polymerization degree
Resin easily decomposed in high temperature.
4) plate resistor is prepared with unleaded encasement medium slurry of anti-acid
Above-mentioned glass dust, inorganic additive are dispersed in by stirring, rolling in organic carrier, have half so as to be prepared into
The unleaded encasement medium slurry of anti-acid of plate resistor is made in the dispersion of fluid viscosity.
Lead-free glass powder
The lead-free glass powder used in the present invention, the inorganic binder help to improve acid resistance and the reduction of plate resistor
Resistance value drift rate.The wherein acid proof mainly glass dust that improves after 600 DEG C of meltings, is closely combined with aluminum oxide substrate,
Glass dust has suitable surface tension after melting simultaneously so that is combined preferably with resistive layer after glass melting, so as to improve
Acid resistance.The wherein reduction of resistance value drift rate mainly since glass dust is after 600 DEG C of meltings, the crystalline solid of formation and resistance
The coefficient of expansion approaches, and the tension on plate resistor surface is reduced, so as to achieve the purpose that protective resistance.
Glass dust percentage composition by weight in the present invention, Bi2O330%~50%, CaO 15%~20%, SiO218%
~25%, ZnO 10%~20%, B2O33%~10%.Wherein Bi2O3The melting temperature of glass dust can be reduced, makes glass dust
More adapt to the sintering process of plate resistor.Wherein CaO can form calcium system glass, solve acidproof sex chromosome mosaicism well.Wherein
ZnO can be formed acicular crystals, solve the problems, such as resistance value drift rate well after sintering.
The effect of glass dust is mainly protection lower resistors, it is necessary to form good bonding with substrate in dielectric paste
Power and make resistance offset excessive with acid resistance, while after cannot being overlapped with resistance.So glass dust in dielectric paste
Content be generally 40%~75%, be preferably 50~65%.
Inorganic additive
Inorganic additive Al in the present invention2O3、ZnO、ZrO2And TiO2In one or several kinds, wherein metal aoxidize
If owner and glass dust form certain specific glass structure in sintering process, so as to improve the items of a packaging slurry
Performance.
These metal oxides can only add one kind, can also the form of mixture add two or more.It is especially excellent
Choosing uses Al2O3, it is contemplated that dispersibility and printing adaptability, the granularity of metal oxide is preferably 0.1 to 8 μm, more preferably
For 0.5 to 5 μm.When granularity is more than 8 μm, cause plug net in easy screen printing process.The inorganic additive in dielectric paste
Content is generally 0.1%~10%, and content is more than that 10% performance that can deteriorate slurry can even influence the radium-shine cutting of R cream, content
The properties of slurry cannot be effectively promoted less than 0.1%, content of the inorganic additive in dielectric paste is preferably 0.1%
To 5%.
Organic carrier
The organic carrier of printing functionality of the present invention is used to implement, mainly inorganic additive and glass dust are mixed well
Together, then it is covered in by silkscreen process on aluminum oxide substrate, then by sintering circuit, realizes glass dust and base
The combination of plate.
Organic carrier percentage composition by weight in the present invention, resin 4%~16%, organic additive 1%~4% have
Solvent 60%~80%;Wherein resin is one or more of rosin resin, ethyl cellulose and methylcellulose.This hair
The preferred rosin resin of resin, ethyl cellulose and methylcellulose in bright, more preferable rosin and ethyl cellulose.It is wherein organic
Solvent is one or more of alcohols or ethers.The preferred alcohols of organic solvent in the present invention or one kind or several in ethers
Kind, more preferable alcohols.
Organic carrier has not significant impact dielectric paste chemical property, and main function is to adjust slurry to suitable
Mobility and net, therefore resin, organic additive and the solvent content in organic carrier are not subject to any specific restrictions excessively, as long as
Content can reach the purpose of the present invention.
In the present invention, above-mentioned glass dust, inorganic additive are dispersed in has by hybrid resin with solvent and what is obtained
In airborne body, so as to prepare with fluid properties slurry.
A kind of unleaded encasement medium slurry of anti-acid of plate resistor of the present invention, can be on plate resistor.
Embodiment
Unless stated otherwise, otherwise the number of expression composition ratio all represents weight percent (weight to following components content
Measure %).
1) glass dust is prepared
An encasement medium slurry in embodiment is made of glass dust, inorganic additive and organic carrier.Slurry glass
The respective content of powder oxide is listed in Table 1 below, and the content of glass dust is set as 65%.
The refining of glass dust is carried out in embodiment using the oxide ratios listed by table 1.
The refining of 1 glass dust of table
2) an encasement medium slurry is prepared
The content of glass dust is set as 65%, inorganic additive Al2O3, content is set as 2%.The content of organic carrier
For 33%.It weighs glass dust, inorganic additive and the various specific amounts of organic carrier and adds in stirrer for mixing, then three
Disperse in roller mill, so as to prepare an encasement medium slurry 1 to 6 according to the formula of size of table 2.
The formula of size of 2 encasement medium slurries of table
Evaluation method
After glass dust, inorganic additive, organic carrier are by three-high mill rolling, slurry basic performance test is carried out.
Slurry is printed to by silk-screen printing on 96% aluminum oxide substrate, drying condition is lower 10 minutes, is then burnt in 600 DEG C of belts
It is sintered in freezing of a furnace with the speed of 120mm/min.Acid resistance test is the substrate that will be obtained in 5%H2SO4It is small that solution impregnates 1
Shi Hou, tap water rinsing, drying are seen to whether there is and are come off with adhesive tape tearing.
Slurry by silk-screen printing is coated on and is overlapped with resistance slurry (resistance value R0) 0603 aluminum oxide substrate on, warp
After crossing 150 DEG C of dryings, 600 DEG C of sintering, the resistance tested at this time is R1, pass through formula (R1-R0)/R0* 100% calculates resistance value
Drift rate.Deviation ratio control is qualification within ± 5% in chip producer.
By encapsulate resistance after dielectric paste it is sintered be placed under metallographic microscope, amplify 100 times, observe dielectric paste
Number of bubbles in surface unit area.Bubble will excessively influence the weather-proof and proof voltage energy of electronic component.
As can be seen that 1 to 4 do not possess acid resistance from the result of the test of table 2;And 1 resistance value drift rate it is excessive, 2 bubble
More, 5 and 6 are provided simultaneously with acid resistance, relatively low resistance value drift rate and less unit area bubble.
Then, further to promote the properties of dielectric paste, the glass dust formula being maintained in slurry 5 and content are not
Become, the content of inorganic additive changes, and then evaluates acid resistance, encapsulating change rate and slurry sintered membrane bubble.Medium slurry
Glass dust, inorganic additive in material 7-12, organic carrier content are shown in Table 3.
The formula of size of the changed encasement medium slurry of content of 3 inorganic additive of table
Use acid resistance, resistance value drift rate and the list of dielectric paste 1-6 evaluation methods measurement dielectric paste described herein
Plane pneumatosis steeps number.For the results show regardless of whether addition inorganic additive, dielectric paste 7-12 has acid resistance, and adds in
Suitable inorganic additive can effectively reduce resistance value drift rate and reduce unit area number of bubbles.
Present disclosure is not limited to cited by embodiment, and those of ordinary skill in the art are by reading description of the invention
And to any equivalent conversion that technical solution of the present invention is taken, it is that claim of the invention is covered.
Claims (8)
1. unleaded encasement medium slurry of anti-acid of plate resistor, it is characterised in that:Percentage composition by weight, including following
Component,
Glass dust 60% ~ 75%, inorganic additive 2% ~ 5%, organic carrier 20% ~ 35%.
2. unleaded encasement medium slurry of anti-acid of plate resistor according to claim 1, it is characterised in that:It is described
Glass dust is Bi-Ca-Si-Zn systems.
3. unleaded encasement medium slurry of anti-acid of plate resistor according to claim 2, it is characterised in that:By weight
Percentage composition is measured, the glass dust includes Bi2O330% ~ 50%, CaO 15% ~ 20%, SiO218% ~ 25%, 10% ~ 20% Hes of ZnO
B2O3 3%~10%。
4. unleaded encasement medium slurry of anti-acid of plate resistor according to claim 1, it is characterised in that:It is described
Inorganic additive is Al2O3、ZnO、ZrO2Or TiO2In one or several kinds.
5. unleaded encasement medium slurry of anti-acid of plate resistor according to claim 1, it is characterised in that:By weight
Percentage composition is measured, the organic carrier includes resin 4% ~ 16%, organic additive 1% ~ 4% and organic solvent 60% ~ 90%.
6. unleaded encasement medium slurry of anti-acid of plate resistor according to claim 5, it is characterised in that:It is described
Resin is one or more of rosin resin, ethyl cellulose or methylcellulose.
7. unleaded encasement medium slurry of anti-acid of plate resistor according to claim 5, it is characterised in that:It is described
Organic solvent is one or both of alcohols or ethers mixture.
8. the plate resistor preparation method of a unleaded encasement medium slurry of anti-acid, which is characterized in that specifically include following
Step:
Prepare glass dust
Percentage composition by weight, by Bi2O330% ~ 50%, CaO 15% ~ 20%, SiO218% ~ 25%, ZnO 10% ~ 20% and B2O3
It is sufficiently mixed with three-dimensional material mixer after 3% ~ 10% weighing, is melted after being taken with corundum crucible Sheng under the conditions of 1000 DEG C ~ 1500 DEG C
Melt, molten liquid is poured into, water quenching is carried out in deionized water at normal temperature, finally by the glass dregs after water quenching through ball milling, drying, sieving one
Glass dust finished product is obtained after series of processes;
Prepare inorganic additive
The inorganic additive is Al2O3、ZnO、ZrO2Or TiO2In one or several kinds, granularity be less than 8 μm, preferred size model
It encloses for 0.5 ~ 5 μm;
Prepare organic carrier
Will percentage composition by weight, the organic carrier include resin 4% ~ 16%, organic additive 1% ~ 4% and organic solvent 60% ~
90% is dissolved and is modulated at 50-150 DEG C, and preferable temperature is 60 DEG C ~ 90 DEG C;
Plate resistor is prepared with unleaded encasement medium slurry of anti-acid
Above-mentioned glass dust, inorganic additive are dispersed in by stirring, rolling in organic carrier, so as to be prepared into semifluid
The unleaded encasement medium slurry of anti-acid of plate resistor is made in the dispersion of viscosity.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110642519A (en) * | 2019-09-25 | 2020-01-03 | 湖南利德电子浆料股份有限公司 | Encapsulation slurry for aluminum nitride substrate and preparation method and application thereof |
CN110683764A (en) * | 2019-11-15 | 2020-01-14 | 黄山市晶特美新材料有限公司 | Glass powder for environment-friendly high-acid-resistance automobile glass slurry and preparation method thereof |
CN111499412A (en) * | 2020-04-02 | 2020-08-07 | 西安宏星电子浆料科技股份有限公司 | Glass paste for thermal printing head and preparation method thereof |
CN113555146A (en) * | 2021-09-22 | 2021-10-26 | 西安宏星电子浆料科技股份有限公司 | High-acid-resistance medium slurry |
CN114530300A (en) * | 2022-04-21 | 2022-05-24 | 西安宏星电子浆料科技股份有限公司 | Lead-free medium slurry |
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CN110642519A (en) * | 2019-09-25 | 2020-01-03 | 湖南利德电子浆料股份有限公司 | Encapsulation slurry for aluminum nitride substrate and preparation method and application thereof |
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CN111499412B (en) * | 2020-04-02 | 2022-10-14 | 西安宏星电子浆料科技股份有限公司 | Glass paste for thermal printing head and preparation method thereof |
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CN114530300A (en) * | 2022-04-21 | 2022-05-24 | 西安宏星电子浆料科技股份有限公司 | Lead-free medium slurry |
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